US3320500A - Tantalum alloy capacitor - Google Patents

Tantalum alloy capacitor Download PDF

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Publication number
US3320500A
US3320500A US516655A US51665565A US3320500A US 3320500 A US3320500 A US 3320500A US 516655 A US516655 A US 516655A US 51665565 A US51665565 A US 51665565A US 3320500 A US3320500 A US 3320500A
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United States
Prior art keywords
tantalum
capacitor
alloy
layer
capacitors
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Expired - Lifetime
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US516655A
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English (en)
Inventor
Norman N Axelrod
Herbert D Guberman
Schwartz Newton
Benjamin H Vromen
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AT&T Corp
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Bell Telephone Laboratories Inc
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Priority to US516655A priority Critical patent/US3320500A/en
Priority to IL26756A priority patent/IL26756A/xx
Priority to FR84555A priority patent/FR1501459A/fr
Priority to BE690127D priority patent/BE690127A/xx
Priority to GB55280/66A priority patent/GB1162709A/en
Priority to DE19661589079 priority patent/DE1589079B2/de
Priority to NL6618117A priority patent/NL6618117A/xx
Application granted granted Critical
Publication of US3320500A publication Critical patent/US3320500A/en
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/002—Details
    • H01G4/005—Electrodes
    • H01G4/008—Selection of materials
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C22C27/02—Alloys based on vanadium, niobium, or tantalum
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/04—Coating on selected surface areas, e.g. using masks
    • C23C14/042—Coating on selected surface areas, e.g. using masks using masks
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/14—Metallic material, boron or silicon
    • C23C14/18—Metallic material, boron or silicon on other inorganic substrates
    • C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/58—After-treatment
    • C23C14/5846—Reactive treatment
    • C23C14/5853—Oxidation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G2/00—Details of capacitors not covered by a single one of groups H01G4/00-H01G11/00

Definitions

  • TANTALUM ALLOY CAPACITOR Filed Dec. 27, 1965 2 Sheets-Sheet 2 g ⁇ l E r -3 3 5 S Q a g 2, 9 $0 a t 6 0 E S g u B? Q 0, Q x t: 2 E u #z 0.; k i. s Q Q Q E S L l 1 l A 520002000 (51 70/1) 39m 70/1 wmoowaaa United States Patent 3,320,500 TANTALUM ALLOY CAPACITOR Norman N. Axelrod, Summit, N.J., Herbert D. Guberman, Oak Ridge, Tenn., and Newton Schwartz, Morris Township, Morris County, and Benjamin H.
  • This invention relates to a technique for the fabrication of a thin film capacitor including an alloy of tantalum as one of the electrodes, an oxide layer of the tantalum alloy as the dielectric and an electrically conductive counter-electrode, and also relates to capacitor-s produced by such technique
  • a technique for the fabrication of a thin film capacitor including an alloy of tantalum as one of the electrodes, an oxide layer of the tantalum alloy as the dielectric and an electrically conductive counter-electrode, and also relates to capacitor-s produced by such technique
  • These structures are typically constructed by depositing a layer of a film forming metal upon a substrate, anodizing the deposited layer to form an oxide film, and finally depositing a counterelectrode in direct contact with the anodized film.
  • the resultant capacitor is polar in nature and represents the first such device in which a semiconductive layer of manganese dioxide is eliminated, such having been a requirement in solid electrolytic capacitors prepared theretofore.
  • a technique for the fabrication of a substantially non-polar capacitor of anodized construction involves modifying the conventional procedure for the fabrication of printed tantalum capacitors by the use of an anode comprising tantalum alloyed with at least one metal selected from among the elements of Groups I(b), II(b), III(a), IV(b), V(b), VI(b) and VIII of the Periodic Table of the Elements (as shown in the 45th edition of the Handbook of Chemistry and Physics, page 'B-2, published by the Chemical Rubber Co., Cleveland, Ohio).
  • the metals of interest herein may be selected from among copper, silver, gold, zinc, cadmium, mercury, aluminum, gallium, indium, thallium, titanium, zirconium, hafnium, vanadium, niobium, chromium, molybdenum, tungsten, iron, cobalt, nickel, ruthenium, rhodium, palladium, osmium, iridium, and platinum.
  • the resultant devices manifest non-polar conduction properties, superior cathodic breakdown voltages, higher initial yields and better life test performance than any of the conventional prior art tantalum capacitors.
  • the substantially non-polar nature of certain of these structures inherently suggests their use in circuits in which polarity changes occur, such as alternating-current circuits, and permits their operation in either direction at voltages ranging up to 30 volts.
  • FIG. 1 is a cross-sectional view of a substrate with a layer of a tantalum alloy deposited thereon;
  • FIG. 2 is a plan view of the body of FIG. 1 after photoengraving and etching to form a desired pattern;
  • FIG. 3 is a plan view of the body of FIG. 2 after anodization
  • FIG. 4 is a plan view of the body of FIG. 3 after the deposition thereon of a counter-electrode;
  • FIG. 5 is a cross-sectional view of the body of FIG. 4.
  • FIG. 6 is a graphical representation on coordinates of breakdown voltage in volts against alloy composition in atom percent showing the enhancement in breakdown voltage evidenced by capacitors produced in accordance with the present invention.
  • FIG. 1 there is shown a substrate 11 upon which a metallic pattern is to be produced in accordance with the present invention.
  • the inventive technique contemplates the use of a substrate material which is able to withstand temperatures to which they may be subjected during the deposition stage of the processing. Glasses and glazed ceramics are particularly suitable in this use.
  • the first step in the inventive technique comprises cleansing the substrate by conventional techniques well known to those skilled in the art.
  • a layer of a tantalum alloy 12 is deposited by conventional procedures, as for example, cathodic sputtering, vacuum evaporation, vapor plating, et cetera, as described by L. Holland in Vacuum Deposition of Thin Films, 1. Wiley and Sons, 1956.
  • This step may conveniently be accomplished by utilizing a tantalum cathode and wrapping thereabout strands of wire of the metal it is desired to alloy with tantalum or a cathode of the alloy.
  • metal-s suitable for use in the present invention may be selected from among the metal elements of Groups I(b), II(b), III(a), IV(b), V(b), VI(b) and VIII of the Periodic Table of the Elements, such elements having been set forth above. Further, it has been determined that in order to obtain the enhanced characteristics, alluded to above, in the resultant capacitors, the metal element must be present in the alloy in an amount ranging from 0.01 to 20.0 atom percent with a preferred range of from 0.1 to 20 atom percent. The noted limits are dictated by practical considerations, namely, the degree of enhancement in characteristics beyond those points. It has been found that the use of amounts less than the noted minimum fails to materially improve operating characteristics beyond those of capacitor grade tantalum. On the other hand, excesses beyond the noted maximum result in a definite degradation of device properties. The preferred range result-s in substantially non-polar devices as well as in superior breakdown characteristics.
  • the minimum thickness of the layer deposited upon the substrate is dependent upon two factors. The first of these is the thickness of the metal which is converted into the oxide form during the subsequent anodizing step. The second factor is the minimum thickness of un-oxidized metal remaining after anodization commensurate with the maximum resistance which can be tolerated in the tantalum alloy electrode. As described herein, the preferred minimum thickness of the tantalum alloy electrode is approximately 2,000 Angstroms. There is no maximum limit on this thickness.
  • an alloy deposit of at least 4,000 Angstroms is preferred. It is considered that of this 4,000 Angstroms a maximum of approximately 1,000 Angstroms is converted during the anodizing step leaving approximately 3,000 Angstroms as the electrode thickness.
  • FIG. 2 is a plain view of substrate 11 showing the pattern resulting from the removal of portions of layer 12.
  • alloy layer 12 is anodized in an appropriate electrolyte, so resulting in an oxide film 13, shown in FIG. 3.
  • Suitable electrolytes for this purpose are phosphoric acid, citric acid, et cetera.
  • the last step in the fabrication of a capacitor in accordance with this invention is the application of a counter-electrode 14, shown in FIG. 4, in contact with the oxide film 13.
  • a counter-electrode 14 shown in FIG. 4
  • Any suitable method for producing an electrically conductive layer on the surface of the oxide layer is suitable, as for example, vacuum evaporation.
  • a cross-sectional view of the finished assembly is shown in FIG. 5. 7
  • Example I A glass slide, approximately one inch in width and three inches in length was cleaned ultrasonically by conventional techniques. Thereafter, a tantalum-molybdenum alloy was deposited upon the cleansed substrate by sputtering techniques.
  • the cathode employed was a 6 x 6" x 050" piece of capacitor grade tantalum ob tained from commercial sources, on strand of molybdenum, obtained from commercial sources, having a diameter of 0.005 inch being wound upon said cathode.
  • Sputtering was effected from both sides of the cathode at4,0 volts and 50 milliamperes in 30 microns of argon for 60 minutes, so resulting in an alloy layer 4,000 Augstroms thick.
  • the resultant layer contained 0.19 atom percent molybdenum.
  • a capacitor pattern was established by means of conventional photoengraving techniques.
  • the capacitor pattern was then anodized in 0.01 weight percent citric acid water solution at a constant current density of one milliampere/cm. until the voltage was 130 volts and then the anodization was continued at constant voltage.
  • the capacitor was removed from the anodizing medium and etched in 0.01 weight percent aluminum chloride in absolute methanol for five seconds with the alloy at a positive potential of 90 volts.
  • the slide was rinsed in alcohol, rinsed in water and re-anodized in citric acid at 130 volts for minutes. Upon completion of the anodiza'tion, the slide was rinsed in distilled water and dried.
  • FIG. 6 there is shown a graphical representation on coordinates of breakdown voltage in vol-ts against alloy composition in atom percent showing variations in anodic and cathodic breakdown volt age as a function of varying molybdenum and iron concentrations in tantalum alloy capacitors.
  • the cathodic or reverse breakdown voltage evidences a significant increase over the compositional range of interest as contrasted with the conventional tantalum capacitor while the non-, catastrophic anodic or forward breakdown voltage remains at a level within the general range of 50-100 volts, such being the required level for diverse device applications.
  • composition-s not only show improved forward and reverse breakdown, but are substantially non-polar.
  • capacitors were formed by sputtering from capacitor grade tantalum cathodes, a tantalum-molybdenum alloy cathode (0.09 atomic percent molybdenum) and a tantalum-molybdenum alloy cathode (0.14 atomic percent molybdenum), and completing the devices as described above. Cathodic breakdown voltages for these devices are shown in Table III.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
US516655A 1965-12-27 1965-12-27 Tantalum alloy capacitor Expired - Lifetime US3320500A (en)

Priority Applications (7)

Application Number Priority Date Filing Date Title
US516655A US3320500A (en) 1965-12-27 1965-12-27 Tantalum alloy capacitor
IL26756A IL26756A (en) 1965-12-27 1966-10-25 Tantalum alloy capacitor and method for the preparation thereof
FR84555A FR1501459A (fr) 1965-12-27 1966-11-22 Condensateur à pellicule mince
BE690127D BE690127A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1965-12-27 1966-11-24
GB55280/66A GB1162709A (en) 1965-12-27 1966-12-09 Thin Film Capacitors
DE19661589079 DE1589079B2 (de) 1965-12-27 1966-12-22 Duennfilmkondensator
NL6618117A NL6618117A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1965-12-27 1966-12-23

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Application Number Priority Date Filing Date Title
US516655A US3320500A (en) 1965-12-27 1965-12-27 Tantalum alloy capacitor

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US3320500A true US3320500A (en) 1967-05-16

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US (1) US3320500A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
BE (1) BE690127A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
DE (1) DE1589079B2 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
FR (1) FR1501459A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
GB (1) GB1162709A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
IL (1) IL26756A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)
NL (1) NL6618117A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html)

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3710474A (en) * 1970-05-22 1973-01-16 Fansteel Inc Vanadium-modified tantalum foil
US3984208A (en) * 1973-02-19 1976-10-05 Societe Lignes Telegraphiques Et Telephoniques Anodes for solid electrolyte capacitors
US4110815A (en) * 1975-10-06 1978-08-29 Societe Lignes Telegraphiques Et Telephoniques Solid electrolytic capacitor
FR2389682A1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) * 1977-05-04 1978-12-01 Siemens Ag
JPS5572026A (en) * 1978-11-25 1980-05-30 Matsushita Electric Ind Co Ltd Method of manufacturing porous electrode for electrolytic condenser
JPS55134925A (en) * 1979-04-10 1980-10-21 Matsushita Electric Ind Co Ltd Sintered electrode for solid electrolytic condenser
US4277543A (en) * 1978-11-25 1981-07-07 Matsushita Electric Industrial Co., Ltd. Anode for solid electrolytic capacitor and method for making the same
US4423087A (en) * 1981-12-28 1983-12-27 International Business Machines Corporation Thin film capacitor with a dual bottom electrode structure
US4471405A (en) * 1981-12-28 1984-09-11 International Business Machines Corporation Thin film capacitor with a dual bottom electrode structure
US4734340A (en) * 1985-07-16 1988-03-29 Sony Corporation Dielectric thin film
US4982309A (en) * 1989-07-17 1991-01-01 National Semiconductor Corporation Electrodes for electrical ceramic oxide devices
US20180132355A1 (en) * 2016-11-04 2018-05-10 Tdk Corporation Thin-film capacitor and electronic component embedded substrate

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2221839B2 (en) † 2000-08-10 2017-05-24 Showa Denko K.K. Niobium powder, sintered body and capacitor using the body

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2299288A (en) * 1940-03-21 1942-10-20 Nat Sugar Refining Company Sugar
US2993266A (en) * 1958-06-16 1961-07-25 Bell Telephone Labor Inc Method of making a capacitor employing film-forming metal electrode
US3203793A (en) * 1963-01-28 1965-08-31 Du Pont Porous columbium and tantalum materials

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2299288A (en) * 1940-03-21 1942-10-20 Nat Sugar Refining Company Sugar
US2993266A (en) * 1958-06-16 1961-07-25 Bell Telephone Labor Inc Method of making a capacitor employing film-forming metal electrode
US3203793A (en) * 1963-01-28 1965-08-31 Du Pont Porous columbium and tantalum materials

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3710474A (en) * 1970-05-22 1973-01-16 Fansteel Inc Vanadium-modified tantalum foil
US3984208A (en) * 1973-02-19 1976-10-05 Societe Lignes Telegraphiques Et Telephoniques Anodes for solid electrolyte capacitors
US4110815A (en) * 1975-10-06 1978-08-29 Societe Lignes Telegraphiques Et Telephoniques Solid electrolytic capacitor
FR2389682A1 (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) * 1977-05-04 1978-12-01 Siemens Ag
US4277543A (en) * 1978-11-25 1981-07-07 Matsushita Electric Industrial Co., Ltd. Anode for solid electrolytic capacitor and method for making the same
JPS5572026A (en) * 1978-11-25 1980-05-30 Matsushita Electric Ind Co Ltd Method of manufacturing porous electrode for electrolytic condenser
JPS55134925A (en) * 1979-04-10 1980-10-21 Matsushita Electric Ind Co Ltd Sintered electrode for solid electrolytic condenser
US4423087A (en) * 1981-12-28 1983-12-27 International Business Machines Corporation Thin film capacitor with a dual bottom electrode structure
US4471405A (en) * 1981-12-28 1984-09-11 International Business Machines Corporation Thin film capacitor with a dual bottom electrode structure
EP0082919A3 (en) * 1981-12-28 1984-09-19 International Business Machines Corporation Thin film capacitor with dual bottom electrode
US4734340A (en) * 1985-07-16 1988-03-29 Sony Corporation Dielectric thin film
US4982309A (en) * 1989-07-17 1991-01-01 National Semiconductor Corporation Electrodes for electrical ceramic oxide devices
US20180132355A1 (en) * 2016-11-04 2018-05-10 Tdk Corporation Thin-film capacitor and electronic component embedded substrate
US10085343B2 (en) * 2016-11-04 2018-09-25 Tdk Corporation Thin-film capacitor and electronic component embedded substrate

Also Published As

Publication number Publication date
GB1162709A (en) 1969-08-27
DE1589079B2 (de) 1972-05-18
NL6618117A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1967-06-28
BE690127A (GUID-C5D7CC26-194C-43D0-91A1-9AE8C70A9BFF.html) 1967-05-02
DE1589079A1 (de) 1970-01-02
FR1501459A (fr) 1967-11-10
IL26756A (en) 1970-07-19

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